Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Sescelades Campus, Marcel·lí Domingo 1, Tarragona 43007, Spain.
Instituto de Investigación para la Gestión Integrada de Zonas Costeras, Campus de Gandia, Universitat Politècnica de València, C/ Paranimf 1, Grao de Gandia, Valencia 46730, Spain.
J Chromatogr A. 2022 Jan 25;1663:462748. doi: 10.1016/j.chroma.2021.462748. Epub 2021 Dec 17.
In this study, the first example of a polytetrafluoroethylene (PTFE)-based magnet coated with weak anion exchange (WAX) monolith as novel support for stir bar sorptive extraction (SBSE) is presented. Firstly, the PTFE magnets were properly modified and vinylized in order to immobilize polymer monoliths onto its surface. Then, a glycidyl methacrylate monolith was prepared and modified with ethylenediamine (EDA) to create weak anion exchanger via ring opening reaction of epoxy groups. The prepared covalently immobilized EDA-modified monoliths onto PTFE magnet exhibited good stability and reusability. Application of resulting material as stir bar for SBSE was investigated for a series of acidic compounds that includes acesulfame, saccharin, diclofenac or ibuprofen, among others as target compounds. Firstly, the SBSE conditions were optimized to promote the WAX interactions with the target compounds achieving recoveries from 37 to 75% and enable the selective extraction of these compounds as it provided values of% matrix effect from 17 to -13% when they were determined by SBSE followed by liquid chromatography - tandem mass spectrometry. The analytical methodology, was then validated and applied for the determination of the target solutes in environmental water samples, which were found at concentration up to 2500 ng L in river waters.
在这项研究中，首次提出了一种基于聚四氟乙烯（PTFE）的涂有弱阴离子交换（WAX）整体柱的磁铁，作为搅拌棒吸附萃取（SBSE）的新型支撑物。首先，对 PTFE 磁铁进行适当的修饰和乙烯化，以便将聚合物整体柱固定在其表面上。然后，制备了甲基丙烯酸缩水甘油酯整体柱，并通过环氧基团的开环反应用乙二胺（EDA）进行改性，以形成弱阴离子交换剂。制备的共价固定化 EDA 改性整体柱在 PTFE 磁铁上表现出良好的稳定性和可重复使用性。将所得材料作为 SBSE 的搅拌棒应用于一系列酸性化合物，包括乙酰磺胺酸、糖精、双氯芬酸或布洛芬等作为目标化合物。首先，优化了 SBSE 条件，以促进 WAX 与目标化合物的相互作用，回收率从 37%到 75%，并能够选择性地萃取这些化合物，因为当它们通过 SBSE 结合液相色谱-串联质谱法进行测定时，基质效应值从 17%到-13%。然后验证并应用该分析方法测定环境水样中的目标溶质，在河水中的浓度高达 2500ng/L。
